CN106581108B - Method for removing residual pesticide propamocarb in ginseng extract - Google Patents
Method for removing residual pesticide propamocarb in ginseng extract Download PDFInfo
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- CN106581108B CN106581108B CN201611233903.XA CN201611233903A CN106581108B CN 106581108 B CN106581108 B CN 106581108B CN 201611233903 A CN201611233903 A CN 201611233903A CN 106581108 B CN106581108 B CN 106581108B
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- ginseng
- propamocarb
- ethyl acetate
- ginseng extract
- petroleum ether
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- 235000020710 ginseng extract Nutrition 0.000 title claims abstract description 19
- WZZLDXDUQPOXNW-UHFFFAOYSA-N propamocarb Chemical compound CCCOC(=O)NCCCN(C)C WZZLDXDUQPOXNW-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 239000005821 Propamocarb Substances 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 title claims abstract description 15
- 239000000575 pesticide Substances 0.000 title claims abstract description 12
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 42
- 241000208340 Araliaceae Species 0.000 claims abstract description 30
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 claims abstract description 30
- 235000003140 Panax quinquefolius Nutrition 0.000 claims abstract description 30
- 235000008434 ginseng Nutrition 0.000 claims abstract description 30
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000003208 petroleum Substances 0.000 claims abstract description 14
- 239000012046 mixed solvent Substances 0.000 claims abstract description 11
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 8
- 230000007935 neutral effect Effects 0.000 claims abstract description 8
- 239000011347 resin Substances 0.000 claims abstract description 8
- 229920005989 resin Polymers 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000001914 filtration Methods 0.000 claims description 8
- 238000009835 boiling Methods 0.000 claims description 7
- 239000000706 filtrate Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 238000000605 extraction Methods 0.000 claims description 4
- 238000010298 pulverizing process Methods 0.000 claims description 4
- 238000000967 suction filtration Methods 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 2
- 238000011084 recovery Methods 0.000 abstract description 7
- 229930182494 ginsenoside Natural products 0.000 abstract description 6
- 229940089161 ginsenoside Drugs 0.000 abstract description 6
- 229930182490 saponin Natural products 0.000 abstract description 3
- 150000007949 saponins Chemical class 0.000 abstract description 3
- 235000017709 saponins Nutrition 0.000 abstract description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 6
- 239000000047 product Substances 0.000 description 3
- XUMBMVFBXHLACL-UHFFFAOYSA-N Melanin Chemical compound O=C1C(=O)C(C2=CNC3=C(C(C(=O)C4=C32)=O)C)=C2C4=CNC2=C1C XUMBMVFBXHLACL-UHFFFAOYSA-N 0.000 description 2
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 2
- 239000000447 pesticide residue Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 150000004657 carbamic acid derivatives Chemical class 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000000817 effect on oomycetes Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000003203 everyday effect Effects 0.000 description 1
- 230000000855 fungicidal effect Effects 0.000 description 1
- 239000000417 fungicide Substances 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 239000003993 organochlorine pesticide Substances 0.000 description 1
- 239000000419 plant extract Substances 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 239000001397 quillaja saponaria molina bark Substances 0.000 description 1
- 230000008326 skin blood flow Effects 0.000 description 1
- 230000037394 skin elasticity Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 230000009885 systemic effect Effects 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/25—Araliaceae (Ginseng family), e.g. ivy, aralia, schefflera or tetrapanax
- A61K36/258—Panax (ginseng)
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation or decoction
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/35—Extraction with lipophilic solvents, e.g. Hexane or petrol ether
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
Landscapes
- Health & Medical Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Life Sciences & Earth Sciences (AREA)
- Microbiology (AREA)
- Pharmacology & Pharmacy (AREA)
- Alternative & Traditional Medicine (AREA)
- Biotechnology (AREA)
- Botany (AREA)
- Medical Informatics (AREA)
- Medicinal Chemistry (AREA)
- Chemical & Material Sciences (AREA)
- Mycology (AREA)
- Engineering & Computer Science (AREA)
- Epidemiology (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Medicines Containing Plant Substances (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention provides a method for removing pesticide propamocarb in a ginseng extract, which is characterized in that according to the property of propamocarb in a ginseng extracting solution, firstly, the propamocarb is extracted by a mixed solvent of petroleum ether and ethyl acetate, then, a mixture of LX-N1, LX-N2 type macroporous resin and 40-60 mesh neutral alumina is filtered, after treatment, the recovery rate of total saponins of ginseng is 80-85%, and the content of propamocarb is less than 0.01 ppm. The method provided by the invention has the advantages of simple operation, low cost, high recovery rate of the total ginsenoside and no unnecessary loss.
Description
Technical Field
The invention belongs to the field of treatment methods of medicinal plant extracts, and particularly relates to a method for removing residual pesticide propamocarb in a ginseng extract.
Background
Ginseng is also called Huangshen, Dijing, Shencao and Baicao king, and is one of the three evergreen plants. Ginseng is a best product for nourishing yin, tonifying life and strengthening body resistance, contains various saponins and polysaccharide components, can be slowly absorbed by skin without adverse stimulation, can expand skin capillary vessels, promote skin blood circulation, increase skin nutrition, regulate water-oil balance of skin, prevent skin dehydration, hardening and wrinkling, and can inhibit the reduction performance of melanin by ginseng active substances, so that the skin is white and smooth, the skin elasticity can be enhanced, cells can be regenerated, and the ginseng skin-care cosmetic is a best product for skin care and beauty. Soaking Ginseng radix directly in 50% glycerol for 10 days, rubbing face with glycerol, or decocting Ginseng radix to obtain concentrated juice, pouring a little of the concentrated juice into face washing water every day, and rubbing face with glycerol containing Ginseng radix or washing face with Ginseng radix water to moisten skin.
However, the ginseng has a long growth cycle, and the ginseng has a large specific surface area and is in direct contact with soil, so that the pesticide residue therein is high, while the ginseng extract is a product after further concentration, and the pesticide residue therein is high.
Propamocarb is a low-toxicity fungicide with a local systemic effect, and belongs to carbamates. Has special effect on oomycetes fungi. It is absorbed by ginseng in soil, and has high concentration after extraction, which is harmful to human body.
In the prior art, the methods for purifying and removing the residual pesticide in the ginseng have certain effect on removing the organochlorine pesticide in the ginseng, but have the defects of high operation pressure, large equipment investment, high operation cost, ginsenoside loss and the like.
Disclosure of Invention
The invention aims to provide a method for removing the residual pesticide propamocarb in a ginseng extract, which has the advantages of simple operation, low cost, high recovery rate of the total ginsenoside and no unnecessary loss.
The invention provides a method for removing pesticide propamocarb residue in a ginseng extract, which comprises the following steps:
1) extracting the ginseng extract with a mixed solvent of petroleum ether and ethyl acetate, and taking the lower layer of feed liquid;
2) then filtering;
3) concentrating the filtrate, and drying.
The preparation method of the ginseng extracting solution in the step 1) comprises the following steps:
pulverizing Ginseng radix, adding into water, heating and boiling, extracting for the first time for 2.5-3.5 hr; adding the residue into water, heating to boil, and extracting for the second time for 1.5-2.5 hr; and combining the two extraction liquid.
Further, the ginseng is crushed and sieved by a 40-60 mesh sieve.
Further, the mass ratio of the ginseng to the water in the first extraction is 1: 7-10; the mass ratio of the ginseng extracted for the second time to the water is 1: 5-8. Further, the vacuum concentration is at 60 ℃; the volume of the filtered liquid after vacuum concentration is 1.5-2.5 times of the mass of the ginseng L/kg.
Further, in the step 1), the volume ratio of the petroleum ether to the ethyl acetate in the mixed solvent of the petroleum ether and the ethyl acetate is 1: 1-2;
the volume ratio of the extracting solution in the step 1) to the mixed solvent of the petroleum ether and the ethyl acetate is 1: 1-2.
Extracting the ginseng extract in the step 1) for 8-10 times by using a mixed solvent of petroleum ether and ethyl acetate.
The filtration in the step 2) is specifically as follows:
mixing the extracted lower layer material liquid with a filter medium, stirring at normal temperature, and performing suction filtration.
Further, the filter medium is a mixture of LX-N1, LX-N2 type macroporous resin and 40-60 mesh neutral alumina according to the mass ratio of 1.5:1.5: 2-2: 2: 1.
Further, the dosage ratio of the lower layer feed liquid to the filter medium in the step 2) is 1.5-2.5L: 50 g.
Further, stirring for 24 hours at normal temperature in the step 2).
Compared with the prior art, the invention aims at the property of propamocarb in the ginseng extract, the mixture of petroleum ether and ethyl acetate is firstly extracted, then the mixture of LX-N1, LX-N2 type macroporous resin and 40-60 mesh neutral alumina is filtered, and after treatment, the recovery rate of the ginseng total saponin is 80-85%, and the propamocarb is less than 0.01 ppm. The method provided by the invention has the advantages of simple operation, low cost, high recovery rate of the total ginsenoside and no unnecessary loss.
Detailed Description
Example 1
A method for removing pesticide propamocarb residue in a ginseng extract comprises the following steps:
1) collecting 1kg of Ginseng radix root hair, pulverizing into 40-60 mesh powder, placing into 15L round bottom flask, adding 7-10L water, heating, extracting for 3 hr from boiling, filtering, and collecting the liquid; adding 5-8L water into the residue, heating, extracting for 2 hr from boiling, filtering, collecting the extractive solution, mixing the extractive solutions, and vacuum concentrating at 60 deg.C to obtain Ginseng radix extractive solution with volume of 1.5-2.5L;
2) using petroleum ether in volume ratio: ethyl acetate ═ 1:1.5, extracting the ginseng extract for 8 times at the same volume and normal temperature by using the mixed solvent, and taking the lower-layer feed liquid;
3) adding 50g of a mixture of LX-N1, LX-N2 type macroporous resin and 40-60 mesh neutral alumina (the mass ratio of LX-N1 to LX-N2 type macroporous resin to 40-60 mesh neutral alumina is 1.5:1.5:2) into the obtained lower layer feed liquid, stirring for 24 hours at normal temperature, and performing suction filtration to obtain a filtrate;
4) concentrating the filtrate at 60 deg.C, and drying.
The recovery rate of the total ginsenoside is 80-85%, and the propamocarb is less than 0.01 ppm.
Example 2
A method for removing pesticide propamocarb residue in a ginseng extract comprises the following steps:
1) collecting 1kg of Ginseng radix root hair, pulverizing into 40-60 mesh powder, placing into 15L round bottom flask, adding 7-10L water, heating, extracting for 3 hr from boiling, filtering, and collecting the liquid; adding 5-8L water into the residue, heating, extracting for 2 hr from boiling, filtering, collecting the extractive solution, mixing the extractive solutions, and vacuum concentrating at 60 deg.C to obtain Ginseng radix extractive solution with volume of 1.5-2.5L;
2) using petroleum ether in volume ratio: ethyl acetate ═ 1:1.5, extracting the ginseng extract for 10 times at the normal temperature by using the mixed solvent with the same volume, and taking the lower-layer feed liquid;
3) adding 50g of a mixture of LX-N1, LX-N2 type macroporous resin and 40-60 mesh neutral alumina (the mass ratio of LX-N1 to LX-N2 type macroporous resin to 40-60 mesh neutral alumina is 2:2:1) into the obtained lower layer feed liquid, stirring for 24 hours at normal temperature, and carrying out suction filtration to obtain a filtrate;
4) concentrating the filtrate at 60 deg.C, and drying.
The recovery rate of the total ginsenoside is 80-85%, and the propamocarb is less than 0.01 ppm.
Claims (3)
1. A method for removing residual pesticide propamocarb in a ginseng extract is characterized by comprising the following steps:
1) extracting the ginseng extract with a mixed solvent of petroleum ether and ethyl acetate, and taking the lower layer of feed liquid;
2) then filtering;
3) concentrating the filtrate, and drying;
in the step 1), the volume ratio of the petroleum ether to the ethyl acetate in the mixed solvent of the petroleum ether and the ethyl acetate is 1: 1.5;
in the step 1), the volume ratio of the extracting solution to the mixed solvent of petroleum ether and ethyl acetate is 1: 1-2;
the preparation method of the ginseng extracting solution in the step 1) comprises the following steps:
pulverizing Ginseng radix, adding into water, boiling, extracting for the first time for 2.5-3.5 hr, adding the residue into water, boiling, extracting for the second time for 1.5-2.5 hr; mixing the two extractive solutions;
the mass ratio of ginseng to water in the first extraction is 1: 7-10; the mass ratio of the ginseng extracted for the second time to the water is 1: 5-8;
the filtration in the step 2) is specifically as follows:
mixing the extracted lower layer feed liquid with a filter medium, stirring at normal temperature, and performing suction filtration;
the filter medium is a mixture of LX-N1, LX-N2 type macroporous resin and 40-60 mesh neutral alumina according to the mass ratio of 1.5:1.5: 2-2: 2: 1.
2. The method for removing propamocarb as a residual pesticide in a ginseng extract according to claim 1, wherein the ginseng extract in the step 1) is extracted with a mixed solvent of petroleum ether and ethyl acetate for 8-10 times.
3. The method for removing the residual pesticide propamocarb in the ginseng extract according to claim 1, wherein the dosage ratio of the lower layer feed liquid to the filter medium in the step 2) is 1.5-2.5L: 50 g.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611233903.XA CN106581108B (en) | 2016-12-28 | 2016-12-28 | Method for removing residual pesticide propamocarb in ginseng extract |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611233903.XA CN106581108B (en) | 2016-12-28 | 2016-12-28 | Method for removing residual pesticide propamocarb in ginseng extract |
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| CN106581108A CN106581108A (en) | 2017-04-26 |
| CN106581108B true CN106581108B (en) | 2020-10-09 |
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| CN112028961A (en) * | 2020-08-17 | 2020-12-04 | 赣州禾绿康健生物技术有限公司 | Method and equipment for removing carbendazim in ginsenoside extract |
| CN112007380B (en) * | 2020-08-23 | 2021-10-22 | 赣州禾绿康健生物技术有限公司 | Device and method for removing residual dimethomorph in ginsenoside extract |
| CN113698987A (en) * | 2021-08-30 | 2021-11-26 | 山东三星玉米产业科技有限公司 | Method for removing residual pesticide in corn oil |
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| CN105777841A (en) * | 2016-04-08 | 2016-07-20 | 赣州禾绿康健生物技术有限公司 | Method for removing propamocarb in araliaceae saponin extract |
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| CN103393928B (en) * | 2013-07-29 | 2015-03-11 | 常熟雷允上制药有限公司 | High-capacity pulse-activating injection and preparation method thereof |
| CN103550273B (en) * | 2013-11-04 | 2016-03-30 | 湖南绿蔓生物科技股份有限公司 | A kind of method extracting the residual ginsenoside of low agriculture from Radix Ginseng |
| CN104490966B (en) * | 2014-12-04 | 2018-01-05 | 宁波中药制药股份有限公司 | A kind of method of remains of pesticide in removing extract of Radix Ginseng stem and leaf |
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| CN105777841A (en) * | 2016-04-08 | 2016-07-20 | 赣州禾绿康健生物技术有限公司 | Method for removing propamocarb in araliaceae saponin extract |
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Denomination of invention: A method for removing residual pesticide shuangmeiwei in ginseng extract Effective date of registration: 20211125 Granted publication date: 20201009 Pledgee: Wuhu Jinsheng Rural Commercial Bank Co.,Ltd. Qingshui sub branch Pledgor: WUHU ACEGEM BIOLOGICAL TECHNOLOGY Co.,Ltd. Registration number: Y2021980013239 |